CN117922146A - Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof - Google Patents

Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof Download PDF

Info

Publication number
CN117922146A
CN117922146A CN202410312686.1A CN202410312686A CN117922146A CN 117922146 A CN117922146 A CN 117922146A CN 202410312686 A CN202410312686 A CN 202410312686A CN 117922146 A CN117922146 A CN 117922146A
Authority
CN
China
Prior art keywords
aerogel film
film
phytic acid
aerogel
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202410312686.1A
Other languages
Chinese (zh)
Inventor
褚夫凯
胡伟兆
宋磊
胡源
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Science and Technology of China USTC
Original Assignee
University of Science and Technology of China USTC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Science and Technology of China USTC filed Critical University of Science and Technology of China USTC
Priority to CN202410312686.1A priority Critical patent/CN117922146A/en
Publication of CN117922146A publication Critical patent/CN117922146A/en
Pending legal-status Critical Current

Links

Abstract

The invention relates to the technical field of aerogel film preparation, and in particular discloses a fire emergency flame-retardant fireproof composite aerogel film, a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, preparing an aromatic polyamide nanofiber solution; s2, preparing a water treatment aerogel film; s3, preparing a phytic acid solution treatment aerogel film; and S4, bonding the phytic acid solution treatment aerogel film in the step S3 on two sides of the water treatment aerogel film in the step S2. The composite aerogel film for fire emergency flame retardance and fire prevention, the preparation method and the application thereof are high in flame retardance level, excellent in heat insulation and fire prevention effect, and convenient to apply to flame retardance and fire prevention of building wooden materials, exterior wall heat insulation materials and building windows when building fires occur.

Description

Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof
Technical Field
The invention relates to the technical field of aerogel film preparation, in particular to a fire emergency flame-retardant fireproof composite aerogel film, a preparation method and application thereof.
Background
In a forest town border area fire, both the flying fire particles and the crown fire heat radiation ignite the combustible and cause the building to catch fire. In the forest and town boundary building, building wood materials, external wall heat insulation materials and building windows are often weak points for causing fire. The flying fire particles and the crown fire heat radiation ignite the wooden material and the outer wall heat insulation material, and the flame of the flying fire particles and the crown fire heat radiation ignites a large amount of heat and toxic smoke; meanwhile, the flying fire particles and the heat radiation of the crown fire easily cause the window glass to break due to the temperature difference, thereby causing the fire disaster in the building. Therefore, there is a need to develop flame retardant, fire resistant, heat insulating materials that are lightweight, easy to deploy, and are used in emergency in border area fires, to delay the development of the fire from forests to buildings.
Aerogels are currently world-recognized solid materials of minimum density, which are of great interest due to their low density, high porosity, and large surface area. The aerogel has various types, and the nano cellulose aerogel, the silicon dioxide aerogel, the graphene aerogel and the like are common.
In the prior art, aerogel can be used as a heat insulation board to be applied to the outer wall of a building to play a role in heat insulation. But lacks an aerogel with heat insulation, flame retardance and high fireproof performance, so that when a fire disaster occurs in a boundary area, the contact between flying fire particles and heat radiation of tree crown fires and building wood materials, external wall heat insulation materials and building windows is blocked.
Disclosure of Invention
The invention aims to provide a fire emergency flame-retardant fireproof composite aerogel film, a preparation method and application thereof, which have high flame-retardant level and excellent heat insulation fireproof effect, and are convenient for flame-retardant fireproof application of building wooden materials, external wall heat insulation materials and building windows when building fires occur.
In order to achieve the above purpose, the invention provides a preparation method of a fire emergency flame-retardant fireproof composite aerogel film, which comprises the following steps:
S1, preparing an aromatic polyamide nanofiber solution;
S2, preparing a water treatment aerogel film;
S3, preparing a phytic acid solution treatment aerogel film;
And S4, bonding the phytic acid solution treatment aerogel film in the step S3 on two sides of the water treatment aerogel film in the step S2.
Preferably, in step S1, the preparation method specifically includes: and adding the aromatic polyamide fiber, the hydrolytic agent and the dimethyl sulfoxide according to a certain proportion, mixing and stirring for 6-12 h to obtain the aromatic polyamide nanofiber solution.
Preferably, the mass ratio of the aromatic polyamide fiber to the hydrolytic agent to the dimethyl sulfoxide is 1:1-1.5:5-6.
Preferably, the aromatic polyamide fiber is one or more of poly (paraphenylene terephthalamide), poly (m-phenylene isophthalamide) fiber or poly (paraphenylene terephthalamide) fiber;
the hydrolytic agent is one of sodium hydroxide or potassium hydroxide.
Preferably, in step S2, the method for preparing the water treatment aerogel film specifically comprises the following steps:
S21, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.25-1 mm, and then placing the die into water to soak for 1-12 h, so as to obtain a hydrogel film with dimethyl sulfoxide removed;
s22, taking out the hydrogel film obtained in the step S21, and freeze-drying to obtain the water treatment aerogel film.
Preferably, in step S3, the method for preparing the phytic acid solution-treated aerogel film specifically comprises the following steps:
S31, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.25-1 mm, and then placing the die into a phytic acid aqueous solution for soaking for 1-12 h to obtain a hydrogel film with molecular chain orientation and dimethyl sulfoxide removal;
S32, taking out the hydrogel film in the step S31, and freeze-drying to obtain the phytic acid solution treated aerogel film.
Preferably, in step S31, the concentration of the phytic acid aqueous solution is 5-30% wt.
Preferably, in step S4, the phytic acid solution treatment aerogel film in step S3 is adhered to both sides of the water treatment aerogel film in step S2 by using an adhesive, wherein the adhesive is one of a polyamide hot melt adhesive, a polyurethane adhesive, an organic silicone adhesive, an epoxy resin adhesive or a polyacrylic resin.
The invention also provides a fire emergency flame-retardant fireproof composite aerogel film prepared by the preparation method, which comprises a water treatment aerogel film of the middle layer and phytic acid treatment aerogel films arranged on two sides of the middle layer, wherein the water treatment aerogel film and the phytic acid treatment aerogel films are bonded.
In order to achieve the purpose, the invention also provides application of the fire emergency flame-retardant fireproof composite aerogel film in the fields of building wooden materials, external wall heat insulation materials and building windows when building fires occur.
Therefore, the invention adopts the fire emergency flame-retardant fireproof composite aerogel film and the preparation method and the application thereof, and has the following technical effects:
(1) The composite aerogel film prepared by the invention has excellent heat insulation, flame retardance and fireproof performance, the aromatic polyamide fiber has good heat resistance and strong chemical stability, and a large number of pore structures are generated in the aerogel film by adopting a water treatment mode, so that the heat conductivity coefficient of the aerogel film is reduced, and the heat insulation capability of the aerogel film is further enhanced; the phytic acid is a natural phosphorus-rich compound, can be used as a flame retardant to promote the generation of a polymer condensed phase carbon layer, and can also be used as a proton donor to regulate and control the molecular chain orientation in the preparation and composition of the aromatic polyamide aerogel. The phytic acid solution is treated to orient the aromatic polyamide nano fibers, so that the fireproof capacity is enhanced, and meanwhile, the introduction of the phosphorus-containing structure greatly enhances the thermal stability and the flame retardance of the aerogel film.
(2) The composite aerogel film prepared by the invention has the characteristics of light weight and easy deployment, and is convenient for emergency fire prevention of building wooden materials, external wall heat insulation materials and building windows when fire occurs.
Drawings
FIG. 1 is a schematic diagram of a fire emergency flame-retardant fireproof composite aerogel film, a preparation method and an application example 1;
FIG. 2 is a drawing of an SEM image of a fire-emergency, flame-retardant, fire-resistant composite aerogel film, a method of making the same, and a water-treated aerogel film of application example 2;
FIG. 3 is a drawing of an SEM (cross-sectional view) of a composite aerogel film for fire emergency, flame retardance and fire prevention, a preparation method and an application of the phytic acid solution of example 3 to treat the aerogel film;
FIG. 4 is a graph showing the temperature-mass residual rate change of the fire emergency flame-retardant fireproof composite aerogel film, the preparation method and the application examples 2 and 4;
FIG. 5 is a graph showing the temperature-mass loss rate of a composite aerogel film for fire emergency, flame retardation and fire prevention of the present invention, and a preparation method and application examples 2 and 4;
FIG. 6 is a graph showing the temperature-heat release rate change of a fire emergency flame retardant and fireproof composite aerogel film, a preparation method and application examples 2 and 4 according to the present invention;
FIG. 7 is a bar graph of thermal conductivity of a fire emergency flame retardant and fire resistant composite aerogel film, method of making and application examples 3 and 4 according to the present invention.
Reference numerals
1. A water treatment aerogel film; 2. treating the aerogel film with a phytic acid solution; 3. and (3) a binder.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1
As shown in figure 1, the fire emergency flame-retardant composite aerogel film comprises a water treatment aerogel film 1 of a middle layer and phytic acid treatment aerogel films 2 arranged on two sides of the middle layer, wherein the water treatment aerogel film 1 and the phytic acid treatment aerogel films 2 are bonded by a bonding agent 3, the whole is layered, and a finished product can be packaged and stored and has the characteristics of light weight and easy deployment.
Example 2
The preparation process of the water treatment aerogel film comprises the following steps:
s1, adding 10g of aromatic polyamide fiber, 12g of potassium hydroxide and 50g of dimethyl sulfoxide, mixing and stirring for 12h, wherein in the process, the potassium hydroxide breaks the imide bond of the aromatic polyamide fiber, and obtaining a new aromatic polyamide nanofiber solution after the chemical reaction is completed.
S2, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.5mm, then placing the die into water for soaking for 10 hours, removing dimethyl sulfoxide by replacement, forming a hydrogel film after replacement, taking out, and freeze-drying to obtain the water treatment aerogel film.
As shown in fig. 2, the water treatment aerogel film exhibited a porous typical aerogel internal morphology, indicating that it had good thermal insulation properties. The water treatment aerogel films alone were tested for no vertical burn rating according to the flammability UL94 rating standard by burn test.
Example 3
The preparation process of the phytic acid solution treated aerogel film comprises the following steps:
S1, adding 10g of aromatic polyamide fiber, 12g of potassium hydroxide and 50g of dimethyl sulfoxide, mixing and stirring for 12h, wherein in the process, the potassium hydroxide breaks imide bonds of the aromatic polyamide fiber, and obtaining a new aromatic polyamide nanofiber solution after the chemical reaction is completed.
S3, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.25mm, then placing the die into a phytic acid aqueous solution with the concentration of 5% wt for soaking for 10 hours, removing dimethyl sulfoxide by replacement, and obtaining the hydrogel film after replacement. At the same time, the aqueous phytic acid solution provides protons to orient the molecular chains in the hydrogel film. Taking out and freeze-drying to obtain the phytic acid solution treated aerogel film.
As shown in fig. 3, phytic acid changes the fiber orientation, and its interior exhibits the characteristic of fiber horizontal orientation. According to the flammability UL94 grade standard, the vertical burning grade of the phytic acid solution treated aerogel film is V0 grade, which shows that the phytic acid obviously enhances the flame retardant property.
Example 4
The preparation process of the composite aerogel film comprises the following steps:
The water-treated aerogel film prepared in example 2 was used as an intermediate layer, and the phytic acid solution-treated aerogel film prepared in example 3 was used as outer layers on both sides of the intermediate layer, and bonded by a polyurethane adhesive to obtain a composite aerogel film having a thickness of 1 mm. The vertical burning rating of the composite aerogel film was V0 rating according to the flammability UL94 rating standard, as tested in example 3.
Example 5
The preparation process of the composite aerogel film comprises the following steps:
S1, unlike in example 2, pouring into a mold with a depth of 0.25mm, and then immersing the mold in water for 5 hours to obtain a water treatment aerogel film.
S2, unlike example 3, pouring into a mold with a depth of 0.25mm, and then immersing the mold in a phytic acid aqueous solution with a concentration of 15% by weight for 12 hours to obtain a phytic acid solution-treated aerogel film.
S3, using the water treatment aerogel film as an intermediate layer and using the phytic acid solution treatment aerogel film as outer layers on two sides of the intermediate layer, and bonding by using a polyurethane adhesive to obtain the composite aerogel film with the thickness of 0.75 mm. The vertical burning grade of the composite aerogel film is V0 grade according to the flammability UL94 grade standard through burning test.
Example 6
The preparation process of the composite aerogel film comprises the following steps:
S1, unlike in example 2, pouring into a mold with a depth of 0.3mm, and then placing the mold in water to soak for 5 hours to obtain a water treatment aerogel film.
S2, unlike example 3, pouring into a mold having a depth of 0.3mm, and then immersing the mold in an aqueous solution of phytic acid having a concentration of 25% by weight for 10 hours to obtain a phytic acid solution-treated aerogel film.
S3, using the water treatment aerogel film as an intermediate layer and using the phytic acid solution treatment aerogel film as outer layers on two sides of the intermediate layer, and bonding by using a polyurethane adhesive to obtain the composite aerogel film with the thickness of 0.9 mm. The vertical burning grade of the composite aerogel film is V0 grade according to the flammability UL94 grade standard through burning test.
Example 7
The preparation process of the composite aerogel film comprises the following steps:
S1, unlike in example 2, pouring into a mold with a depth of 0.5mm, and then placing the mold in water to soak for 5 hours to obtain a water treatment aerogel film.
S2, unlike example 3, pouring into a mold having a depth of 0.3mm, and then immersing the mold in a phytic acid aqueous solution having a concentration of 30% by weight for 12 hours to obtain a phytic acid solution-treated aerogel film.
S3, using the water treatment aerogel film as an intermediate layer and using the phytic acid solution treatment aerogel film as outer layers on two sides of the intermediate layer, and bonding by using a polyurethane adhesive to obtain the composite aerogel film with the thickness of 1.1 mm. The vertical burning grade of the composite aerogel film is V0 grade according to the flammability UL94 grade standard through burning test.
Test
Thermal stability test of example 2 and example 4:
As shown in fig. 4 and 5, the mass residual rate and the mass loss rate of the water treatment aerogel film and the composite aerogel film under an air atmosphere were obtained by using a differential thermal analyzer, respectively. The carbon residue (mass residue) of the water treatment aerogel film of example 2 at 800 ℃ was 11wt%, and the carbon residue of the composite aerogel film of example 4 at 800 ℃ was significantly raised to 54wt%. It is demonstrated that the high temperature thermal stability of the composite aerogel film is significantly improved compared to the water treatment aerogel film. Meanwhile, the mass loss rate of the composite aerogel film is obviously reduced, and the results show that the introduction of the phytic acid obviously enhances the high-temperature carbonizing capability of the composite aerogel film.
Heat release behavior test of example 2 and example 4:
As shown in fig. 6, the heat release rates of the water treatment aerogel film and the composite aerogel film were obtained using an external igniter. The maximum heat release rate of the water treatment aerogel film of example 2 was 208W/g, and the maximum heat release rate of the composite aerogel film of example 4 was only 54W/g. It was demonstrated that the heat release rate of the composite aerogel film was significantly suppressed compared to the water treatment aerogel film.
Thermal conductivity test of example 3 and example 4:
as shown in fig. 7, the thermal conductivity of the phytic acid treated aerogel film and the composite aerogel film were measured using a thermal protection plate method thermal conductivity meter. The phytic acid solution treated aerogel film of example 3 had a thermal conductivity of 0.062w.m -1.K-1 and the composite aerogel film of example 4 had a thermal conductivity of 0.052w.m -1.K-1. The water treatment aerogel film of the middle layer is used, so that the heat conductivity coefficient of the composite aerogel film is reduced, and the heat insulation capability of the composite aerogel film is improved.
Fire test of examples 2 and 4-7:
By adopting an alcohol lamp fire prevention test, the composite aerogel films prepared in the examples 4-7 can not burn through within 10min, and the water treatment aerogel film prepared in the example 2 can burn through when contacting flame. The composite aerogel film has excellent fireproof capability.
Therefore, the composite aerogel film for fire emergency flame retardance and fire prevention, the preparation method and the application thereof are high in flame retardance level, excellent in heat insulation and fire prevention effect, and convenient to apply to flame retardance and fire prevention of building wooden materials, external wall heat insulation materials and building windows when building fires occur.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.

Claims (7)

1. The preparation method of the fire emergency flame-retardant fireproof composite aerogel film is characterized by comprising the following steps of:
S1, preparing an aromatic polyamide nanofiber solution;
S2, preparing a water treatment aerogel film;
S3, preparing a phytic acid solution treatment aerogel film;
S4, bonding the phytic acid solution treatment aerogel film in the step S3 on two sides of the water treatment aerogel film in the step S2;
in step S2, the method for preparing the water treatment aerogel film specifically comprises the following steps:
S21, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.25-1 mm, and then placing the die into water to soak for 1-12 h, so as to obtain a hydrogel film with dimethyl sulfoxide removed;
S22, taking out the hydrogel film obtained in the step S21, and freeze-drying to obtain a water treatment aerogel film;
in step S3, the method for preparing the phytic acid solution-treated aerogel film specifically comprises the following steps:
s31, pouring the aromatic polyamide nanofiber solution obtained in the step S1 into a die with the depth of 0.25-1 mm, and then placing the die into a phytic acid aqueous solution for soaking for 1-12 h to obtain a hydrogel film with molecular chain orientation and dimethyl sulfoxide removal;
S32, taking out the hydrogel film obtained in the step S31, and freeze-drying to obtain a phytic acid solution treated aerogel film;
In step S4, the phytic acid solution treatment aerogel film in step S3 is adhered to both sides of the water treatment aerogel film in step S2 by using an adhesive, wherein the adhesive is one of a polyamide hot melt adhesive, a polyurethane adhesive, an organic silica gel adhesive, an epoxy resin adhesive or a polyacrylic resin.
2. The preparation method of the fire emergency flame-retardant fireproof composite aerogel film according to claim 1, wherein in the step S1, the preparation method specifically comprises the following steps: and adding the aromatic polyamide fiber, the hydrolytic agent and the dimethyl sulfoxide according to a certain proportion, mixing and stirring for 6-12 h to obtain the aromatic polyamide nanofiber solution.
3. The preparation method of the fire emergency flame-retardant fireproof composite aerogel film according to claim 2, wherein the mass ratio of the aromatic polyamide fiber to the hydrolytic agent to the dimethyl sulfoxide is 1:1-1.5:5-6.
4. The method for preparing a fire emergency flame-retardant fireproof composite aerogel film according to claim 2, wherein the aromatic polyamide fiber is one or more of poly (paraphenylene terephthalamide), poly (m-phenylene isophthalamide) fiber or poly (parabenzamide) fiber;
the hydrolytic agent is one of sodium hydroxide or potassium hydroxide.
5. The method for preparing a fire emergency flame-retardant fireproof composite aerogel film according to claim 1, wherein in the step S31, the concentration of the phytic acid aqueous solution is 5-30% wt.
6. A fire emergency flame-retardant fireproof composite aerogel film prepared by the preparation method according to any one of claims 1 to 5, which comprises a water treatment aerogel film of an intermediate layer and phytic acid treatment aerogel films arranged on two sides of the intermediate layer, wherein the water treatment aerogel film and the phytic acid treatment aerogel films are bonded.
7. Use of the fire emergency fire-retardant fire-resistant composite aerogel film according to claim 6 in the fields of building wood materials, exterior wall insulation materials and building windows in the event of a building fire.
CN202410312686.1A 2024-03-19 2024-03-19 Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof Pending CN117922146A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202410312686.1A CN117922146A (en) 2024-03-19 2024-03-19 Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202410312686.1A CN117922146A (en) 2024-03-19 2024-03-19 Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN117922146A true CN117922146A (en) 2024-04-26

Family

ID=90766650

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202410312686.1A Pending CN117922146A (en) 2024-03-19 2024-03-19 Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN117922146A (en)

Similar Documents

Publication Publication Date Title
Xie et al. A highly efficient flame retardant nacre-inspired nanocoating with ultrasensitive fire-warning and self-healing capabilities
CN109370288B (en) Intumescent water-based fireproof flame-retardant coating for wood material and preparation method thereof
CN101565625B (en) Silicone rubber fireproof sealing material and preparation method thereof
CN110628077B (en) Flame-retardant smoke-suppressing flexible polyurethane foam composite material and preparation method thereof
EA003177B1 (en) Fire retardant intumescent coating for lignocellulosic materials
JP7473123B2 (en) Fire-retardant laminate and method for producing the same
FI99021C (en) Thermally expandable fire protection compound
CN113150235B (en) Expandable graphite hard polyurethane composite thermal insulation material and preparation method thereof
Zhang et al. A self-healing, recyclable, and degradable fire-retardant gelatin-based biogel coating for green buildings
KR101812203B1 (en) The eco-friendly inorganic flame retardant adhesive composition
WO2021135723A1 (en) Single-component non-flammable polyurethane fire protection paint and preparation method thereof
KR101618654B1 (en) Fire Prevention Net coated Fire-Retardant Material of Environment Friendly and None Toxic Intumescent
KR101589060B1 (en) Environment Friendly and None Toxic Intumescent Fire-Retardant Paint
CN105038238A (en) Preparation method of organic silicon fire retardant of organic silicon rubber wastes
CN117922146A (en) Fire emergency flame-retardant fireproof composite aerogel film, and preparation method and application thereof
KR20190068453A (en) Non-combustible thermal insulation
KR20090019407A (en) Fire retardant polystyrene foam and sandwich panel using thereof
CN116396656A (en) Composite fireproof paint and preparation method thereof
KR101979449B1 (en) Fire Retardant Coating Composition insulater
KR101448253B1 (en) Intumescence fireproof coating composition with ligneous cellulose fiber
CN109401406B (en) Intumescent smoke-suppressing fire retardant for water-based paint and preparation method thereof
CN112375257B (en) Efficient environment-friendly composite flame retardant and preparation method thereof
Harun-Ur-Rashid et al. Fire-Resistant Polymeric Foams and Their Applications
CN113582655A (en) Expandable flexible fireproof material and preparation method thereof
CN113249004A (en) Water-based intumescent fire retardant coating for galvanized steel sheet and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination